Large and Pressure-Dependent c-Axis Piezoresistivity of Highly Oriented Pyrolytic Graphite near Zero Pressure.

The c-axis piezoresistivity is a fundamental and important parameter of graphite, but its value near zero pressure has not been well determined. Herein, a new method for studying the c-axis piezoresistivity of van der Waals materials near zero pressure is developed on the basis of in situ scanning electron microscopy and finite element simulation. The c-axis piezoresistivity of microscale highly oriented pyrolytic graphite (HOPG) is found to show a large value of 5.68 × 10-5 kPa-1 near zero pressure and decreases by 2 orders of magnitude to the established value of ∼10-7 kPa-1 when the pressure increases to 200 MPa. By modulating the serial tunneling barrier model on the basis of the stacking faults, we describe the c-axis electrical transport of HOPG under compression. The large c-axis piezoresistivity near zero pressure and its large decrease in magnitude with pressure are attributed to the rapid stiffening of the electromechanical properties under compression.

Atomistic Investigation of Grain Boundary Fracture in Alumina.

Grain boundary (GB) fracture is a major mechanism of material failure in polycrystalline ceramics. However, the intricate atomic arrangements of GBs have impeded our understanding of the atomistic mechanisms of these processes. In this study, we investigated the atomic-scale crack propagation behavior of an α-Al2O3 ∑13 grain boundary, using a combination of in situ transmission electron microscopy (TEM) and scanning TEM. The atomic-scale fracture path along the GB core was directly determined by the observation of the atomic structures of the fractured surfaces, which is consistent with density functional theory calculations. We found that the GB fracture can be attributed to the weaker local bonds and a smaller number of bonds along the fracture path. Our findings provide atomistic insights into the mechanisms of crack propagation along GBs, offering significant implications for GB engineering and the toughening of ceramics.

Automated High-Throughput Atomic Force Microscopy Single-Cell Nanomechanical Assay Enabled by Deep Learning-Based Optical Image Recognition.

Mechanical forces are essential for life activities, and the mechanical phenotypes of single cells are increasingly gaining attention. Atomic force microscopy (AFM) has been a standard method for single-cell nanomechanical assays, but its efficiency is limited due to its reliance on manual operation. Here, we present a study of deep learning image recognition-assisted AFM that enables automated high-throughput single-cell nanomechanical measurements. On the basis of the label-free identification of the cell structures and the AFM probe in optical bright-field images as well as the consequent automated movement of the sample stage and AFM probe, the AFM probe tip could be accurately and sequentially moved onto the specific parts of individual living cells to perform a single-cell indentation assay or single-cell force spectroscopy in a time-efficient manner. The study illustrates a promising method based on deep learning for achieving operator-independent high-throughput AFM single-cell nanomechanics, which will benefit the application of AFM in mechanobiology.

Indentation Depth-Dependent Hardness of Metal-Organic Framework Crystals: The Effect of Local Amorphization Induced by Indentation.

The hardness of metal-organic frameworks (MOFs) is an important mechanical property metric measuring their resistance to the permanent plastic deformation. The hardness of most MOFs measured from nanoindentation experiments usually exhibits the similar unique indentation depth dependence feature, the mechanism of which still remains unclear. In order to explain the effect of the indentation depth on the hardness of MOFs, we conducted nanoindentation simulations on HKUST-1 by using reactive molecular dynamics simulations. Our simulations reveal that the HKUST-1 material near the indenter can transform from the parent crystalline phase to a new amorphous phase due to the high pressure generated, while its counterpart far from the indenter remains in the crystalline phase. By considering the crystalline-amorphous interface in the energy analysis of MOFs, we derived an analytical expression of the hardness at different indentation depths. It is found that the interface effect can greatly increase the hardness of MOFs, as observed in nanoindentation simulations. Moreover, the proposed analytical expression can well explain the indentation depth-dependent hardness of many MOF crystals measured in nanoindentation experiments. Overall, this work can provide a better understanding of the indentation depth dependence of the hardness of MOFs.

Exploring the origins of the indentation size effect at submicron scales.

The origin of the indentation size effect has been extensively researched over the last three decades, following the establishment of nanoindentation as a broadly used small-scale mechanical testing technique that enables hardness measurements at submicrometer scales. However, a mechanistic understanding of the indentation size effect based on direct experimental observations at the dislocation level remains limited due to difficulties in observing and quantifying the dislocation structures that form underneath indents using conventional microscopy techniques. Here, we employ precession electron beam diffraction microscopy to "look beneath the surface," revealing the dislocation characteristics (e.g., distribution and total length) as a function of indentation depth for a single crystal of nickel. At smaller depths, individual dislocation lines can be resolved, and the dislocation distribution is quite diffuse. The indentation size effect deviates from the Nix-Gao model and is controlled by dislocation source starvation, as the dislocations are very mobile and glide away from the indented zone, leaving behind a relatively low dislocation density in the plastically deformed volume. At larger depths, dislocations become highly entangled and self-arrange to form subgrain boundaries. In this depth range, the Nix-Gao model provides a rational description because the entanglements and subgrain boundaries effectively confine dislocation movement to a small hemispherical volume beneath the contact impression, leading to dislocation interaction hardening. The work highlights the critical role of dislocation structural development in the small-scale mechanistic transition in indentation size effect and its importance in understanding the plastic deformation of materials at the submicron scale.

An attempt to identify brain tumour tissue in neurosurgery by mechanical indentation measurements.

BACKGROUND: The intraoperative differentiation between tumour tissue, healthy brain tissue, and any sensitive structure of the central nervous system is carried out in modern neurosurgery using various multimodal technologies such as neuronavigation, fluorescent dyes, intraoperative ultrasound or the use of intraoperative MRI, but also the haptic experience of the neurosurgeon. Supporting the surgeon by developing instruments with integrated haptics could provide a further objective dimension in the intraoperative recognition of healthy and diseased tissue. METHODS: In this study, we describe intraoperative mechanical indentation measurements of human brain tissue samples of different tumours taken during neurosurgical operation and measured directly in the operating theatre, in a time frame of maximum five minutes. We present an overview of the Young's modulus for the different brain tumour entities and potentially differentiation between them. RESULTS: We examined 238 samples of 75 tumour removals. Neither a clear distinction of tumour tissue against healthy brain tissue, nor differentiation of different tumour entities was possible on solely the Young's modulus. Correlation between the stiffness grading of the surgeon and our measurements could be found. CONCLUSION: The mechanical behaviour of brain tumours given by the measured Young's modulus corresponds well to the stiffness assessment of the neurosurgeon and can be a great tool for further information on mechanical characteristics of brain tumour tissue. Nevertheless, our findings imply that the information gained through indentation is limited.

Raman spectroscopic measurements and imaging on sub-newton Berkovich and spherical imprints in fused silica.

This paper lays out best practices for evaluating and optimizing a Raman spectroscopy setup to ensure the collection of reliable spectral data and/or Raman images on indented glasses. The Raman spectroscopic measurements and imaging were conducted on residual imprints created with Berkovich and spherical probes at forces in the sub-newton range in fused silica. The capability of a conventional optical instrument for mapping spectral variations in sub-newton imprints on glasses is evaluated by studying the influence of the optical configuration (choice of microscope objective) on the spatial resolution of the spectroscopy setup. The spatial resolution was quantitatively assessed in Z profile measurements and qualitatively evaluated by mapping changes in spectral features and correlated densification within the indented regions of fused silica specimens. The paper discusses the importance of appropriately matching the analysis volume of the Raman spectroscopic setup with the size of the indentation-induced densification zone by demonstrating the detrimental effects a mismatch may have on accurately capturing the magnitude of spectral changes and correlated densification.

A Comprehensive Review on the Viscoelastic Parameters Used for Engineering Materials, Including Soft Materials, and the Relationships between Different Damping Parameters.

Although the physical properties of a structure, such as stiffness, can be determined using some statical tests, the identification of damping parameters requires a dynamic test. In general, both theoretical prediction and experimental identification of damping are quite difficult. There are many different techniques available for damping identification, and each method gives a different damping parameter. The dynamic indentation method, rheometry, atomic force microscopy, and resonant vibration tests are commonly used to identify the damping of materials, including soft materials. While the viscous damping ratio, loss factor, complex modulus, and viscosity are quite common to describe the damping of materials, there are also other parameters, such as the specific damping capacity, loss angle, half-power bandwidth, and logarithmic decrement, to describe the damping of various materials. Often, one of these parameters is measured, and the measured parameter needs to be converted into another damping parameter for comparison purposes. In this review, the theoretical derivations of different parameters for the description and quantification of damping and their relationships are presented. The expressions for both high damping and low damping are included and evaluated. This study is considered as the first comprehensive review article presenting the theoretical derivations of a large number of damping parameters and the relationships among many damping parameters, with a quantitative evaluation of accurate and approximate formulas. This paper could be a primary resource for damping research and teaching.

Effect of heat treatment and nitrogen atmosphere during post-curing on mechanical properties of 3D-printed orthodontic aligners.

OBJECTIVES: Three-dimensional (3D)-printed aligners present a promising orthodontic treatment modality, whose clinical success largely depends on the material's mechanical properties. The aim of this study was to evaluate the mechanical properties of resin-made 3D-printed aligners and assess the effect of two different post-curing conditions. MATERIALS AND METHODS: Forty dumbbell-shaped specimens and 40 resin aligners were 3D-printed and divided into four equal groups according to post-curing conditions: presence or absence of oxygen during post-curing and water heat treatment at 85°C for 15 s or none. Samples from the central incisor of the aligner (n = 5/group) were studied by Attenuated Total Reflection Fourier-transform infrared spectroscopy (ATR-FTIR). The dumbbell-shaped specimens were loaded up to fracture under tensile mode and yield strength, ultimate tensile strength, elastic and plastic strain were calculated. The first mandibular molar area from 3D-printed aligners (n = 10/group) was cut and embedded in acrylic resin and then underwent metallographic grinding and polishing followed by instrumented indentation testing to determine the following mechanical properties: Martens hardness, indentation modulus, elastic index, and indentation relaxation. After descriptive statistics, differences according to each post-curing protocol, as well as their combination, were analyzed with linear regression modeling at a 5% significance level. RESULTS: All groups showed identical ATR-FTIR spectra, while no statistically significant effects were seen for either post-curing protocol (N2 presence and heat treatment) or their combination (P > .05 in all instances). CONCLUSIONS: The mechanical properties of 3D-printed resin aligners were not considerably affected either by post-curing in N2 atmosphere or heat treatment.

Irradiation-Hardening Model of TiZrHfNbMo0.1 Refractory High-Entropy Alloys.

In order to find more excellent structural materials resistant to radiation damage, high-entropy alloys (HEAs) have been developed due to their characteristics of limited point defect diffusion such as lattice distortion and slow diffusion. Specially, refractory high-entropy alloys (RHEAs) that can adapt to a high-temperature environment are badly needed. In this study, TiZrHfNbMo0.1 RHEAs are selected for irradiation and nanoindentation experiments. We combined the mechanistic model for the depth-dependent hardness of ion-irradiated metals and the introduction of the scale factor f to modify the irradiation-hardening model in order to better describe the nanoindentation indentation process in the irradiated layer. Finally, it can be found that, with the increase in irradiation dose, a more serious lattice distortion caused by a higher defect density limits the expansion of the plastic zone.

[Study on methods measuring mechanical properties of arterial wall by macroscopic indentation].

Accurately evaluating the local biomechanics of arterial wall is crucial for diagnosing and treating arterial diseases. Indentation measurement can be used to evaluate the local mechanical properties of the artery. However, the effects of the indenter's geometric structure and the analysis theory on measurement results remain uncertain. In this paper, four kinds of indenters were used to measure the pulmonary aorta, the proximal thoracic aorta and the distal thoracic aorta in pigs, and the arterial elastic modulus was calculated by Sneddon and Sirghi theory to explore the influence of the indenter geometry and analysis theory on the measured elastic modulus. The results showed that the arterial elastic modulus measured by cylindrical indenter was lower than that measured by spherical indenter. In addition, compared with the calculated results of Sirghi theory, the Sneddon theory, which does not take adhesion forces in account, resulted in slightly larger elastic modulus values. In conclusion, this study provides parametric support for effective measurement of arterial local mechanical properties by millimeter indentation technique.

Photomodulation of the Mechanical Properties and Photo-Actuation of Chitosan-Based Thin Films Modified with an Azobenzene-Derivative.

A sophisticated comprehension of the impacts of photoisomerization and photothermal phenomena on biogenic and responsive materials can provide a guiding framework for future applications. Herein, the procedure to manufacture homogeneous chitosan-based smart thin films are reported by incorporating the light-responsive azobenzene-derivative Sodium-4-[(4-(2-(2-(2-methoxyethoxy)ethoxy)ethoxy)phenyl)diazen-yl]-benzenesulfonate (TEGABS) in the biopolymer through electrostatic interactions. When irradiated with UV-light the TEGABS/chitosan films show a biresponse, comprising the E→Z photoisomerization with a half-life of 13 - 20 h and the light-induced evaporation of residual moisture leading to an increase in the reduced indentation modulus (up to 49%) and hardness. Freestanding films of TEGABS/chitosan show actuation up to 13° while irradiated with UV-light. This work shows the potential of biogenic polysaccharides in the design of biresponsive materials with photomodulated mechanical properties and unveils the link between the humidity of the environment, residual moisture, and the photomodulation of the mechanical properties.

Analysis of biomechanical properties of mouse skin dermis through atomic force microscopy: Application to demonstrate a sexual dimorphism.

An in-depth understanding of the mechanical properties of the dermis is indispensable to improve wound healing or slow-down skin ageing. Despite crucial research issues for dermatological and cosmetic industries, very little is known about the mechanical behaviour of the dermis at nanoscale level. This knowledge is relevant not only to human skin but also to mouse skin since this animal model is widely used in basic and preclinical studies for skin biology and health. Here, we describe an original protocol that we developed to specifically measure the mechanical properties of mouse dermis using atomic force microscopy-based nano-indentation approach. Using horizontal cryosections (i.e. parallel to the skin surface) performed at different depths through the dermis of dorsal skin, our protocol allowed us to detect nanoscale mechanical changes between female and male dermis samples. We found that the dermis was softer (i) in females than in males and (ii) with depth within the dermis of male mice. We also quantified compositional differences between female and male skin dermis and found that increased extracellular matrix gene expression and type V collagen staining were associated with increased dermal stiffness in male mice, compared with females. Our results demonstrating a sexual dimorphism in the nanomechanical properties and molecular composition of mouse dermis, open the way to better consider sex-related cutaneous differences to understand skin disease and to stimulate the development of female versus male-specific products with more appropriate dermatological treatments and cosmetic interventions.

Mechanical resilience of the sessile tunicate Botryllus schlosseri.

We demonstrate that the sessile tunicate Botryllus schlosseri is remarkably resilient to applied loads by attaching the animals to an extensile substrate subjected to quasistatic equiradial loads. Animals can withstand radial extension of the substrate to strain values as high as 20% before they spontaneously detach. In the small to moderate strain regime, we found no relationship between the dynamic size of the external vascular bed and the magnitude of applied stretch, despite known force sensitivities of the vascular tissue at the cellular level. We attribute this resilience to the presence and mechanical properties of the tunic, the cellulose-enriched gel-like substance that encases the animal bodies and surrounding vasculature.

In situthermal noise measurements under nanoindentation of suspended graphene.

We demonstrated thermal noise measurement under the nanoindentation of monolayer and bilayer graphene nanodrums. The resonant oscillation of the cantilever excited only by a thermal energy is detectable even in the case of contact with a suspended graphene. The contact resonance fRequency can be obtained in 1 millisecond intervals during the force curve measurement by optimizing the parameters of a real-time spectrum analyzer. The pretension value of the graphene nanodrum is evaluated by the minimum frequency just when the applied force of the cantilever becomes zero. The simultaneous measurement of the force and the resonant frequency with respect to the deformation of the graphene nanodrum enables us to determine the value of InvOLS (inverse optical lever sensitivity) more accurately in each measurement. From the analysis scheme, force curve measurements of the graphene nanodrums with the same diameters show good reproducibility. We also revealed that the effective spring constant of the graphene nanodrums consists of a weak sample-dependent pretension factor and a deformation-dependent factor proportional to the number of graphene layers.

Nanoindentation of embedded particles.

We address the effect of elastic inhomogeneity on elastic modulus and hardness determinations made by depth-sensing indentations performed on individual particles embedded within a matrix of different elastic modulus. Finite element simulations and nanoindentation experiments are used to quantify the consequences of particle/matrix elastic inhomogeneity and we propose an adaptation of the Oliver-Pharr method that gives access to particle properties knowing those of the matrix. The method is suitable for any combination of matrix and particle elastic modulus and for any type of indenter, provided that the area of the tested particles along the surface of the sample is measured and that a large number of particles are probed. Further conditions for the implementation of the method are that testing conditions be such (i) that permanent deformation of the matrix is avoided, and (ii) that permanent deformation in each probed particle under the indenter is not affected by the matrix.

Precise determination of Young's modulus of amorphous CuZr/nanocrystalline Cu multilayer via nanoindentation.

Extracting mechanical data of thin films on rigid substrates using nanoindentation is compromised by the mechanical properties of underlying substrates, which may falsify the obtained results. With ongoing miniaturization, the substrate influence becomes more pronounced. In this study we present an experimental approach to extract the true Young's modulus of crystalline-amorphous multilayers by means of nanoindentation. We used 1 µm thick multilayers comprised of amorphous CuZr and nanocrystalline Cu. All films were deposited onto two rigid substrate types with Young's moduli below and above the ones expected for the deposits (film-to-substrate hardness and elastic moduli ratios between 0.3 to 1.1 and 0.6 to 1.5, respectively). Linear extrapolation of indentation data to zero indentation depth allows to precisely determine the real film's Young's modulus. Same investigations were performed on monolithic Cu and CuZr films of same thickness. While the hardness values change with the variation of the bilayer thickness of the multilayer structures, the Young's modulus is not affected by the interfaces.

Spatial and Temporal Mapping of Articular Cartilage Poro-Viscoelastic Material Properties Using Indentation.

Biphasic poro-viscoelastic constitutive material model (BPVE) captures both the fluid flow dependent and independent behavior of cartilage under stress relaxation type indentation. A finite element model based on BPVE formulation was developed to explore the sensitivity of the model to Young's modulus, Poisson's ratio, permeability, and viscoelastic constitutive parameters expressed in terms of Prony series coefficients. Then we fit the numerical model to experimental force versus time curves from stress relaxation indents on bovine tibial plateaus to extract the material properties. Measurements were made over the period of two days to capture the material property changes that resulted from trypsin-induced degradation. We measured spatial and temporal changes in mechanical properties in the cartilage. The areas of degradation were characterized by an increase in both permeability and summation of Prony series shear relaxation amplitude constants. These findings suggest that cartilage degradation reduces the intrinsic viscoelastic properties of the solid phase of the tissue in addition to impairing its capacity to offer frictional drag to the interstitial fluid flow (permeability). The changes in material properties are measurable well before structural degradation occurs.

Observation of indentation-induced shear bands in a metal-organic framework glass.

Metal-organic framework (MOF) glasses are a newly emerged family of melt-quenched glasses. Recently, several intriguing features, such as ultrahigh glass-forming ability and low liquid fragility, have been discovered in a number of zeolitic imidazolate frameworks (ZIFs) that are a subset of MOFs. However, the fracture behavior of ZIF glasses has not been explored. Here we report an observation of both cracking pattern and shear bands induced by indentation in a representative melt-quenched ZIF glass, that is, ZIF-62 glass (ZnIm1.68bIm0.32). The shear banding in the ZIF glass is in strong contrast to the cracking behavior of other types of fully polymerized glasses, which do not exhibit any shear bands under indentation. We attribute this anomalous cracking behavior to the easy breakage of the coordinative bonds (Zn-N) in ZIF glasses, since these bonds are much weaker than the ionic and covalent bonds in network glasses.

Mapping stress inside living cells by atomic force microscopy in response to environmental stimuli.

The response of cells to environmental stimuli, under either physiological or pathological conditions, plays a key role in determining cell fate toward either adaptive survival or controlled death. The efficiency of such a feedback mechanism is closely related to the most challenging human diseases, including cancer. Since cellular responses are implemented through physical forces exerted on intracellular components, more detailed knowledge of force distribution through modern imaging techniques is needed to ensure a mechanistic understanding of these forces. In this work, we mapped these intracellular forces at a whole-cell scale and with submicron resolution to correlate intracellular force distribution to the cytoskeletal structures. Furthermore, we visualized dynamic mechanical responses of the cells adapting to environmental modulations in situ. Such task was achieved by using an informatics-assisted atomic force microscope (AFM) indentation technique where a key step was Markov-chain Monte Carlo optimization to search for both the models used to fit indentation force-displacement curves and probe geometry descriptors. We demonstrated force dynamics within cytoskeleton, as well as nucleoskeleton in living cells which were subjected to mechanical state modulation: myosin motor inhibition, micro-compression stimulation and geometrical confinement manipulation. Our results highlight the alteration in the intracellular prestress to attenuate environmental stimuli; to involve in cellular survival against mechanical signal-initiated death during cancer growth and metastasis; and to initiate cell migration.